CN105798544A - Tungsten-copper composite material and preparation method thereof - Google Patents

Tungsten-copper composite material and preparation method thereof Download PDF

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Publication number
CN105798544A
CN105798544A CN201410853498.6A CN201410853498A CN105798544A CN 105798544 A CN105798544 A CN 105798544A CN 201410853498 A CN201410853498 A CN 201410853498A CN 105798544 A CN105798544 A CN 105798544A
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copper
tungsten
carbon
composite material
plate
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CN201410853498.6A
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CN105798544B (en
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惠志林
周增林
李艳
林晨光
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GRIMN Engineering Technology Research Institute Co Ltd
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The invention discloses a tungsten-copper composite material and a preparation method thereof and belongs to the technical field of composite materials. According to the invention, the method comprises the following steps: firstly, enabling copper to infiltrate to the surface layer or the interior of a base material by adopting a copper infiltration method by taking a tungsten plate with a porous structure as the base material; secondly, carrying out electrodeposition copper cladding on a tungsten copper plate or a tungsten copper-tungsten-tungsten copper plate by adopting a pulse power supply in a rotating device after surface treatment; and finally, carrying out rolling leveling and annealing treatment to obtain the tungsten-copper composite material. The tungsten-copper composite material is a laminated composite metal sheet. According to the invention, electrodeposition copper cladding is carried out on the tungsten copper plate or the tungsten copper-tungsten-tungsten copper plate by adopting the pulse power supply in the rotating device, the clad copper layer is good in uniformity, intra-plate deviation is within 10%; metallic copper is good in combination effect with the base material, the copper layer is controllable in thickness, and the yield is high; and the tungsten-copper composite material prepared according to the invention can be widely applied to the fields of electronics, electric equipment, aerospace, machinery and the like.

Description

A kind of tungsten-carbon/carbon-copper composite material and preparation method thereof
Technical field
The invention belongs to technical field of composite materials, be specifically related to a kind of tungsten-carbon/carbon-copper composite material and preparation method thereof.
Background technology
There is tungsten and the respective characteristic of copper and advantage due to tungsten-carbon/carbon-copper composite material, the excellent specific property of high-melting-point tungsten and high heat-conductivity conducting metallic copper, namely high elevated temperature strength, high electrical and thermal conductivity, good electrical erosion resistance, higher hardness, low thermal coefficient of expansion and there is the characteristics such as certain plasticity, can adjusting its corresponding machinery and physical property by change group element ratio, therefore this composite can be widely applied to the fields such as electronics, electrical equipment, space flight, machinery.
Prepare the method that the method majority of lamination composition metal plate adopts Rolling compund at present, it is exactly the both sides that by the method for Rolling compund, metal such as copper is compound in core with metallic plate such as binary metal or unit metal for core, make, by big drafts, a kind of complex method that each constituent element layer combines, therefore there is the shortcomings such as the layering low, easy of material interface bond strength, lumber recovery be low.
Summary of the invention
It is an object of the invention to, overcome above-mentioned the deficiencies in the prior art, it is provided that a kind of tungsten-carbon/carbon-copper composite material and preparation method thereof.Tungsten-the carbon/carbon-copper composite material of the present invention is lamination composition metal plate, the method for the present invention have metallic copper and base material in conjunction with feature effective, that copper layer thickness is controlled, lumber recovery is high.
To achieve these goals, the technical solution used in the present invention is:
The preparation method of a kind of tungsten-carbon/carbon-copper composite material, comprises the following steps:
(1) tungsten plate is oozed copper, obtain copper tungsten plate or tungsten copper-tungsten-copper tungsten plate;
(2) copper tungsten plate or tungsten copper-tungsten-copper tungsten plate are carried out surface treatment;
(3) pulse power electrodeposition in copper tungsten plate or tungsten copper-tungsten-copper tungsten plate is adopted to cover copper in the rotating device;
(4) tungsten-carbon/carbon-copper composite material is obtained through rolling leveling and annealing.
Wherein,
Tungsten plate described in step (1) is loose structure, and porosity is 7~30%, and thickness is 0.1~100.0mm.
Ooze the method for copper described in step (1) for putting copper in tungsten plate both sides, make copper penetrate into tungsten plate top layer or inside, time 0.1~5h under the non-oxidizing atmosphere of 1100~1500 DEG C.
Further, described copper is copper coin, Copper Foil, copper wire or copper rod.
Surface treatment described in step (2) is finishing, cleaning and ion copper facing.
Further, described cleaning is soak 3~180 seconds in the hydrochloric acid of volume ratio 5~50%, then rinses with clear water.
Further, the copper-plated copper layer thickness of described ion is 0.01~50 μm.
Negative electrode in rotary apparatus described in step (3) carries out rotation and revolution relative to anode, and rotating speed is 0~100rpm, and rotating is spaced apart 0~60 second.
Annealing described in step (4) is constant temperature 0.2~3h under the non-oxidizing atmosphere of 350~1000 DEG C.
The consumption of copper and overall dimensions when the present invention oozes copper, ooze component content and distribution that the porosity of copper temperature, time and tungsten plate determines that copper penetrates in tungsten layer, i.e. the content of copper and depth of penetration, distribution in tungsten-copper alloy.Finishing is that copper tungsten plate or tungsten copper-tungsten-copper tungsten plate surface irregularity part give polishing grinding leveling, removes its attachment and makes copper tungsten plate or tungsten copper-tungsten-copper tungsten plate thickness uniform, and makes its surface clean and tidy.Rolling leveling is the copper tungsten plate after electrodeposition covers copper or the concordance being improved layers of copper on tungsten copper-tungsten-copper tungsten plate composite by rolling further, controls thickness, increases the combination of copper and base material, improves the compactness of copper, fineness and flatness.
The present invention also provides for tungsten-carbon/carbon-copper composite material prepared by a kind of said method.
Beneficial effects of the present invention:
The present invention adopts pulse power electrodeposition in copper tungsten plate or tungsten copper-tungsten-copper tungsten plate to cover copper in the rotating device, and institute's copper clad layers uniformity is good, with plate difference within 10%;Metallic copper and base material in conjunction with effective, copper layer thickness is uniform, controlled, and lumber recovery is high;Tungsten-carbon/carbon-copper composite material prepared by the present invention can be widely applied to the fields such as electronics, electrical equipment, space flight, machinery.
Accompanying drawing explanation
Fig. 1 is the sectional schematic diagram of the tungsten-carbon/carbon-copper composite material of embodiment 1 preparation;Wherein, 1-layers of copper, 2-tungsten-copper alloy layer.
Fig. 2 is the sectional schematic diagram of the tungsten-carbon/carbon-copper composite material of embodiment 2 preparation;Wherein, 1-layers of copper, 2-tungsten-copper alloy layer, 3-tungsten layer.
Detailed description of the invention
Below in conjunction with specific embodiments and the drawings, the present invention will be further described, but it is not intended that limiting the scope of the invention.Some nonessential improvement and adjustment that the present invention is done by any one skilled in the art according to the invention described above content, all should be encompassed within protection scope of the present invention.
Embodiment 1
First select 2 porositys 25%, overall dimensions 60 × 200mm, thick 2.4mm tungsten plate as base material, stove is put into, constant temperature 1.5h under the hydrogen atmosphere of 1250 DEG C after the copper rod of Φ 3 × 200mm being respectively placed in the upper and lower both sides of tungsten plate and fastening with the copper wire of Φ 1mm;Secondly, being immersed in the hydrochloric acid of 40% (volume ratio) again 30 seconds after oozing 2 tungsten plate polishing grindings of copper, taking-up clear water is rinsed well, is dried, and utilizes the layers of copper of ion copper coating plating thick layer 0.1 μm;Then in the rotary apparatus that the degree of depth is 350mm (liquid level distance bottom), the copper tungsten plate of 2 diverse locations is carried out electrodeposition with the pulse power simultaneously cover copper, namely acid copper sulfate solution self-loopa at room temperature carries out, CuSO4·H2O:195g/L, H2SO4: the rotating speed 10rpm of 55g/L, rotation and revolution, 5 seconds, rotating interval, pulse frequency 100HZ, pulse current 20A, dutycycle 40%, time 4h, cover the layers of copper of copper after testing with plate difference within 5%;Finally utilize double-roll rolling mill at room temperature to roll for 2.5mm with thickness requirement, and constant temperature 1h is annealed processing under the hydrogen atmosphere of 600 DEG C.
The composite of above-mentioned preparation is copper-tungsten copper-copper, and interface bond strength is not less than 200Mpa, and its sectional schematic diagram is as shown in Figure 1.
Embodiment 2
First select 2 porositys 10%, overall dimensions 60 × 200mm, thick 4.8mm tungsten plate as base material, take Copper Foil identical with tungsten plate overall dimensions, thick 0.2mm and be respectively placed in the upper and lower both sides of tungsten plate, stove is put into, constant temperature 0.5h under the hydrogen atmosphere of 1150 DEG C after fastening with the copper wire less than Φ 1mm;Secondly, being immersed in the hydrochloric acid of 20% (volume ratio) again 60 seconds after oozing 2 tungsten plate polishing grindings of copper, taking-up clear water is rinsed well, is dried, and utilizes the layers of copper of ion copper coating plating thick layer 3 μm;Then in the rotary apparatus that the degree of depth is 350mm (liquid level distance bottom), the copper tungsten plate of 2 diverse locations is carried out electrodeposition with the pulse power simultaneously cover copper, namely acid copper sulfate solution self-loopa at room temperature carries out, CuSO4·H2O:190g/L, H2SO4: the rotating speed 20rpm of 52g/L, rotation and revolution, 10 seconds, rotating interval, pulse frequency 100HZ, pulse current 16A, dutycycle 60%, time 5h, cover the layers of copper of copper after testing with plate difference within 10%;Finally utilize double-roll rolling mill at room temperature to roll for 5.0mm with thickness requirement, and constant temperature 0.5h is annealed processing under the hydrogen atmosphere of 900 DEG C.
The composite of above-mentioned preparation is copper-tungsten copper-tungsten-tungsten copper-copper, and interface bond strength is not less than 200Mpa, and its sectional schematic diagram is as shown in Figure 2.

Claims (10)

1. the preparation method of tungsten-carbon/carbon-copper composite material, it is characterised in that comprise the following steps:
(1) tungsten plate is oozed copper, obtain copper tungsten plate or tungsten copper-tungsten-copper tungsten plate;
(2) copper tungsten plate or tungsten copper-tungsten-copper tungsten plate are carried out surface treatment;
(3) pulse power electrodeposition in copper tungsten plate or tungsten copper-tungsten-copper tungsten plate is adopted to cover copper in the rotating device;
(4) tungsten-carbon/carbon-copper composite material is obtained through rolling leveling and annealing.
2. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 1, it is characterised in that tungsten plate described in step (1) is loose structure, and porosity is 7~30%, and thickness is 0.1~100.0mm.
3. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 1, it is characterized in that, ooze the method for copper described in step (1) for putting copper in tungsten plate both sides, make copper penetrate into tungsten plate top layer or inside, time 0.1~5h under the non-oxidizing atmosphere of 1100~1500 DEG C.
4. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 3, it is characterised in that described copper is copper coin, Copper Foil, copper wire or copper rod.
5. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 1, it is characterised in that the surface treatment described in step (2) is finishing, cleaning and ion copper facing.
6. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 5, it is characterised in that described cleaning is soak 3~180 seconds in the hydrochloric acid of volume ratio 5~50%, then rinses with clear water.
7. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 5, it is characterised in that the copper-plated copper layer thickness of described ion is 0.01~50 μm.
8. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 1, it is characterised in that the negative electrode in rotary apparatus described in step (3) carries out rotation and revolution relative to anode, and rotating speed is 0~100rpm, and rotating is spaced apart 0~60 second.
9. the preparation method of a kind of tungsten-carbon/carbon-copper composite material according to claim 1, it is characterised in that annealing described in step (4) is constant temperature 0.2~3h under the non-oxidizing atmosphere of 350~1000 DEG C.
10. a kind of tungsten-carbon/carbon-copper composite material that prepared by the arbitrary described method of claim 1-9.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111993755A (en) * 2020-08-24 2020-11-27 河北工业大学 Preparation method of magnesium/iron bimetal multilayer composite board
CN112975307A (en) * 2021-05-11 2021-06-18 陕西斯瑞新材料股份有限公司 Method for improving brazing strength of tungsten-copper part
CN114769598A (en) * 2022-04-28 2022-07-22 安庆帝伯粉末冶金有限公司 Valve guide copper infiltration sintering method

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111993755A (en) * 2020-08-24 2020-11-27 河北工业大学 Preparation method of magnesium/iron bimetal multilayer composite board
CN112975307A (en) * 2021-05-11 2021-06-18 陕西斯瑞新材料股份有限公司 Method for improving brazing strength of tungsten-copper part
CN112975307B (en) * 2021-05-11 2021-07-30 陕西斯瑞新材料股份有限公司 Method for improving brazing strength of tungsten-copper part
CN114769598A (en) * 2022-04-28 2022-07-22 安庆帝伯粉末冶金有限公司 Valve guide copper infiltration sintering method
CN114769598B (en) * 2022-04-28 2024-04-09 安庆帝伯粉末冶金有限公司 Copper-infiltration sintering method for valve guide pipe

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